CN112731174B - Method for evaluating full-charge and shallow-discharge performance of lithium battery positive electrode material - Google Patents
Method for evaluating full-charge and shallow-discharge performance of lithium battery positive electrode material Download PDFInfo
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/385—Arrangements for measuring battery or accumulator variables
- G01R31/3865—Arrangements for measuring battery or accumulator variables related to manufacture, e.g. testing after manufacture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The application discloses an evaluation method of high-temperature full-charge shallow-discharge performance of a lithium battery positive electrode material, which comprises the following steps: the method comprises the following steps: preparing a lithium battery anode material into a battery; step two: charging a battery to about 100% soc; discharging the battery to a target SoC with a preset discharge rate current; repeating for n times; step three: collecting the dissolved matter of the battery, and judging the full charge and shallow discharge performance of the lithium battery anode material according to the content of metal elements in the dissolved matter; wherein the target SoC is 80-98%, and n is more than or equal to 50 and less than or equal to 500. For a fixed battery system (a negative electrode, electrolyte and other technical parameters are the same), the full charge and shallow discharge performance of a positive electrode material has obvious correlation with the dissolution amount of metal elements in the positive electrode material, so that the full charge and shallow discharge performance of the positive electrode material can be predicted through the dissolution amount in a fixed cycle, and the cycle of full charge and shallow discharge is not required to be repeated until gas is generated after the positive electrode material is made into a battery.
Description
Technical Field
The application relates to the technical field of lithium batteries, in particular to a method for evaluating high-temperature full-charge and shallow-discharge performance of a lithium battery positive electrode material.
Background
The lithium ion battery has high energy density, long cycle life and good safety, and is widely applied to consumer electronic products such as mobile phones, notebook computers, bluetooth headsets and the like. According to the characteristics of actual use conditions, the consumer electronic products have high requirements on the full charge and shallow discharge performance of the lithium battery in a high-temperature environment, and do not generate gas after being subjected to multiple cycle tests. Among various components of lithium ion batteries, the performance of the positive electrode material plays a key role in the high-temperature full-charge and shallow-discharge performance of the battery. The anode material is in a high-temperature and high-SoC state for a long time in the test process, and the structural stability is influenced, so that the battery generates gas. However, the cycle test of the full charge and shallow discharge performance is long, and when different anode materials are selected for comparison, the experiment is difficult to be completed quickly, and the development progress of the product is influenced. However, no evaluation method specially aiming at the full charge and shallow discharge performance of the positive electrode material exists in the industry, so that a method capable of quickly evaluating the full charge and shallow discharge performance of the positive electrode material of the lithium battery is needed.
Disclosure of Invention
The present application is directed to solving at least one of the problems in the prior art. Therefore, the application provides a method for rapidly evaluating the full charge and shallow discharge performance of the lithium battery positive electrode material.
In a first aspect of the present application, a method for evaluating high-temperature full-charge and shallow-discharge performance of a lithium battery positive electrode material is provided, and the method comprises the following steps:
the method comprises the following steps: preparing a lithium battery anode material into a battery;
step two: charging the battery to about 100% soc; discharging the battery to a target SoC with a preset discharge rate current; repeating for n times;
step three: collecting the dissolved matter of the battery, and judging the full charge and shallow discharge performance of the lithium battery anode material according to the content of metal elements in the dissolved matter;
wherein the target SoC is 80-98%, and n is more than or equal to 50 and less than or equal to 500.
According to the evaluation method of the embodiment of the application, at least the following beneficial effects are achieved:
the existing evaluation method for the full-charge shallow-discharge performance is to judge through gas generation when a battery fails, but the gas generation is rapidly generated when the cycle number of the full-charge shallow-discharge reaches a threshold value, and the prejudgment is poor. The inventors have surprisingly found that, for a fixed battery system (a negative electrode, an electrolyte and other technical parameters are the same), the full charge and shallow discharge performance of a positive electrode material has a relatively obvious correlation with the dissolution amount of metal elements in the positive electrode material, so that the full charge and shallow discharge performance of the positive electrode material can be predicted by fixing the dissolution amount in a week without repeating the full charge and shallow discharge cycle until gas is generated after the positive electrode material is made into a battery.
The existing lithium battery anode material comprises lithium cobaltate, lithium manganate, lithium iron phosphate, lithium titanate, ternary polymers (such as lithium nickel cobalt manganese oxide and lithium nickel cobalt aluminate), other lithium-rich materials, modified materials/mixed materials of the materials and the like. The metal element in the above evaluation method means a metal element other than lithium in these positive electrode materials.
According to some embodiments of the application, the method of charging the battery to 100% soc is: and charging the battery to an upper limit voltage at a constant current with a preset charging rate current, and then charging the battery to a cut-off current at a constant voltage.
According to some embodiments of the present application, the charge rate current is 0.2C to 1.5C.
According to some embodiments of the present application, the charge rate current is 0.5C to 1.0C.
According to some embodiments of the application, the upper voltage is 4.2V to 4.6V.
According to some embodiments of the application, the upper voltage is 4.3V to 4.5V.
According to some embodiments of the present application, the off-current is 0.01C to 0.1C.
According to some embodiments of the present application, the off-current is 0.02C to 0.05C.
According to some embodiments of the present application, the discharge-rate current is between 0.01C and 0.5C.
According to some embodiments of the present application, the discharge rate current is between 0.02C and 0.2C.
According to some embodiments of the present application, step two is performed at a temperature of 35 ℃ to 60 ℃.
According to some embodiments of the present application, step two is performed at a temperature of 45 ℃ to 55 ℃.
According to some embodiments of the present application, in the second step, the charging is performed to 100% SoC and then the standing is performed for 1min to 20min, and the discharging is performed to the target SoC and then the standing is performed for 1min to 20min.
According to some embodiments of the present application, in the second step, the battery is left to stand for 5min to 15min after being charged to 100% SoC, and is left to stand for 5min to 15min after being discharged to the target SoC.
According to some embodiments of the application, the battery is a half-cell. Full charge and shallow discharge performance test in order to detect gas generation, the positive electrode material is generally prepared into a soft package full cell. When the evaluation method is adopted, the battery can be directly prepared into a half battery, and the detection process is effectively shortened.
According to some embodiments of the present application, the battery is a button half cell.
According to some embodiments of the application, the method of collecting the eluate of the battery is: and disassembling the battery, and cleaning the battery component by using an organic solvent to obtain a solution of a dissolved matter.
According to some embodiments of the present application, the organic solvent is selected from at least one of ethylene carbonate, dimethyl carbonate, diethyl carbonate, propylene carbonate, ethyl methyl carbonate.
According to some embodiments of the present application, the battery is discharged to 2.5V to 3.5V before the eluate of the battery is collected.
According to some embodiments of the present application, the method of detecting the metal element is inductively coupled plasma atomic emission spectrometry (ICP method).
According to some embodiments of the present application, the metallic element is selected from at least one of nickel, cobalt, manganese.
Additional aspects and advantages of the present application will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the present application.
Detailed Description
The conception and the resulting technical effects of the present application will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, and not all embodiments, and other embodiments obtained by those skilled in the art without inventive efforts based on the embodiments of the present application belong to the protection scope of the present application.
The following detailed description of the embodiments of the present application is exemplary and is intended to be illustrative of the application and is not to be construed as limiting the application.
In the description of the present application, the meaning of a plurality is one or more, the meaning of a plurality is two or more, and the above, below, exceeding, etc. are understood as excluding the present number, and the above, below, within, etc. are understood as including the present number. If there is a description of first and second for the purpose of distinguishing technical features only, this is not to be understood as indicating or implying a relative importance or implicitly indicating the number of technical features indicated or implicitly indicating the precedence of technical features indicated.
In the description of the present application, unless otherwise specifically limited, terms such as set, installed, connected and the like should be understood broadly, and those skilled in the art can reasonably determine the specific meanings of the above terms in the present application in combination with the specific contents of the technical solutions.
In the description of the present application, reference to the description of the terms "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Example 1
The embodiment provides a method for evaluating the full charge and shallow discharge performance of a lithium battery positive electrode material, which comprises the following steps of:
the method comprises the following steps: preparation of half-cells
Will be obtained by different preparation processesTo LiCoO 2 Uniformly mixing the positive electrode slurry with conductive carbon black (super P), a binder polyvinylidene fluoride (PVDF) and a solvent N-methylpyrrolidone (NMP) according to a certain proportion to prepare the positive electrode slurry. Wherein LiCoO is used as a carrier 2 The mass fraction of (B) is 80-95 wt%.
And coating the positive electrode slurry on an aluminum foil according to a certain surface density and drying to obtain the positive electrode plate. And rolling the positive plate according to a certain compaction density, and punching the positive plate into a wafer by using a punching machine.
Assembling the positive electrode wafer, the diaphragm, the lithium sheet, the gasket, the elastic sheet, the electrolyte and the like into a button type half cell, and activating under the normal temperature condition.
Step two: full charge and shallow discharge cycle
The button half cell was placed in a 45 ℃ incubator. Charging to an upper limit voltage of 4.45V by adopting a charging rate current of 0.5C and constant current, then charging to a cut-off current of 0.05C by adopting constant voltage so as to enable the SoC to reach about 100%, and standing for 10min; discharging with 0.05C discharge rate current for 60min to 95% target SoC, standing for 10min; the above operation of this step was repeated 100 times.
Step three: collection and detection of dissolved-out material
Disassembling the button type half cell in a glove box, cleaning the inner sides of a positive shell and a negative shell of the button type half cell, a gasket, a spring plate, a diaphragm, a lithium plate, a positive pole piece and other button type half cell components by using 50mL dimethyl carbonate (DMC), and collecting cleaning liquid, namely solution of dissolved substances.
Transferring the solution of the dissolved substance to a volumetric flask, adding dimethyl carbonate to achieve a constant volume of 100mL, and detecting the Co content in the solution after constant volume by using an inductively coupled plasma emission spectrometer.
Example 2
This example provides a method for evaluating the full charge and shallow discharge performance of a lithium battery positive electrode material, which is different from example 1 in that the temperature condition of full charge and shallow discharge is set to 55 ℃. The method comprises the following specific steps:
the method comprises the following steps: preparation of half-cells
LiCoO obtained by different preparation processes 2 Mixing with conductive carbon black (super P), polyvinylidene fluoride (PVDF) as binder, and N-methylpyrrolidone as solvent(NMP) is mixed evenly according to a certain proportion to prepare anode slurry. Wherein LiCoO is used as a carrier 2 The mass fraction of (B) is 80-95 wt%.
And coating the positive electrode slurry on an aluminum foil according to a certain surface density and drying to obtain the positive electrode plate. And rolling the positive plate according to a certain compaction density, and punching the positive plate into a wafer by using a punching machine.
Assembling the positive electrode wafer, the diaphragm, the lithium sheet, the gasket, the elastic sheet, the electrolyte and the like into a button type half cell, and activating under the normal temperature condition.
Step two: full charge and shallow discharge cycle
The button half-cell was placed in a 55 ℃ incubator. Charging to an upper limit voltage of 4.45V by adopting a charging rate current of 0.5C and constant current, then charging to a cut-off current of 0.05C by adopting constant voltage so as to enable the SoC to reach about 100%, and standing for 10min; discharging with 0.05C discharge rate current for 60min to 95% target SoC, standing for 10min; this step operation was repeated 100 times.
Step three: collection and detection of dissolved-out material
Disassembling the button type half cell in a glove box, cleaning the inner sides of a positive shell and a negative shell of the button type half cell, a gasket, a spring plate, a diaphragm, a lithium plate, a positive pole piece and other button type half cell components by using 50mL dimethyl carbonate (DMC), and collecting cleaning liquid, namely solution of dissolved substances.
Transferring the solution of the dissolved substance to a volumetric flask, adding dimethyl carbonate to achieve a constant volume of 100mL, and detecting the Co content in the solution after constant volume by using an inductively coupled plasma emission spectrometer.
Example 3
This example provides a method for evaluating the full charge and shallow discharge performance of a lithium battery positive electrode material, which is different from example 2 in that the upper limit voltage of the full charge and shallow discharge is increased to 4.5V. The method comprises the following specific steps:
the method comprises the following steps: preparation of half-cells
LiCoO2 obtained by different preparation processes is uniformly mixed with conductive carbon black (super P), a binder polyvinylidene fluoride (PVDF) and a solvent N-methylpyrrolidone (NMP) according to a certain proportion to prepare anode slurry. Wherein the mass fraction of LiCoO2 is 80-95 wt%.
And coating the positive electrode slurry on an aluminum foil according to a certain surface density and drying to obtain the positive electrode plate. And rolling the positive plate according to a certain compaction density, and punching the positive plate into a wafer by using a punching machine.
Assembling the positive electrode wafer, the diaphragm, the lithium sheet, the gasket, the elastic sheet, the electrolyte and the like into a button type half cell, and activating under the normal temperature condition.
Step two: full charge and shallow discharge cycle
The button half-cell was placed in a 55 ℃ incubator. Charging to the upper limit voltage of 4.5V by adopting a charging rate current of 0.5C and constant current, then charging to the cut-off current of 0.05C by adopting constant voltage so as to enable the SoC to reach about 100%, and standing for 10min; discharging with 0.05C discharge rate current for 60min to 95% target SoC, standing for 10min; this step operation was repeated 100 times.
Step three: collection and detection of dissolved-out material
Disassembling the button type half cell in a glove box, cleaning the inner sides of a positive shell and a negative shell of the button type half cell, a gasket, a spring plate, a diaphragm, a lithium plate, a positive pole piece and other button type half cell components by using 50mL dimethyl carbonate (DMC), and collecting cleaning liquid, namely solution of dissolved substances.
Transferring the solution of the dissolved substance to a volumetric flask, adding dimethyl carbonate to achieve a constant volume of 100mL, and detecting the Co content in the solution after constant volume by using an inductively coupled plasma emission spectrometer.
Example 4
This example provides a method for evaluating the full charge and shallow discharge performance of a lithium battery positive electrode material, which is different from example 3 in that the cycle number of full charge and shallow discharge is 200. The method comprises the following specific steps:
the method comprises the following steps: preparation of half-cells
LiCoO obtained by different preparation processes 2 Uniformly mixing the positive electrode slurry with conductive carbon black (super P), a binder polyvinylidene fluoride (PVDF) and a solvent N-methylpyrrolidone (NMP) according to a certain proportion to prepare the positive electrode slurry. Wherein LiCoO 2 The mass fraction of (B) is 80-95 wt%.
And coating the positive electrode slurry on an aluminum foil according to a certain surface density and drying to obtain the positive electrode plate. And rolling the positive plate according to a certain compaction density, and punching the positive plate into a wafer by using a punching machine.
Assembling the positive electrode wafer, the diaphragm, the lithium sheet, the gasket, the elastic sheet, the electrolyte and the like into a button type half cell, and activating under the normal temperature condition.
Step two: full charge and shallow discharge cycle
The button half-cell was placed in a 55 ℃ incubator. Charging to an upper limit voltage of 4.45V by adopting a charging rate current of 0.5C and constant current, then charging to a cut-off current of 0.05C by adopting constant voltage so as to enable the SoC to reach about 100%, and standing for 10min; discharging with 0.05C discharge rate current for 60min to 95% target SoC, standing for 10min; this step operation was repeated 200 times.
Step three: collection and detection of dissolved-out material
Disassembling the button half-cell in a glove box, cleaning the button half-cell components such as the inner sides of a positive shell and a negative shell, a gasket, a spring plate, a diaphragm, a lithium plate, a positive pole piece and the like of the button half-cell by using 50mL dimethyl carbonate (DMC), and collecting cleaning liquid, namely solution of a dissolved substance.
Transferring the solution of the dissolved matter to a volumetric flask, adding dimethyl carbonate to achieve a constant volume of 100mL, and detecting the Co content in the solution after the constant volume by adopting an inductively coupled plasma emission spectrometer.
Comparative test
Comparative example 1
The comparative example is a method for detecting the full charge and shallow discharge performance of a lithium battery anode material, and comprises the following steps:
the method comprises the following steps: preparation of soft package full battery
LiCoO obtained by different preparation processes 2 Uniformly mixing the positive electrode slurry with conductive carbon black (super P), a binder polyvinylidene fluoride (PVDF) and a solvent N-methylpyrrolidone (NMP) according to a certain proportion to prepare the positive electrode slurry. Wherein LiCoO is used as a carrier 2 The mass fraction of (B) is 80-95 wt%.
And coating the positive electrode slurry on an aluminum foil according to a certain surface density and drying to obtain the positive electrode plate. And rolling the positive plate according to a certain compaction density, and punching the positive plate into a wafer by using a punching machine.
A pouch full cell was prepared using the same electrolyte and separator as in example 1, with graphite as the negative electrode. Each positive electrode material was 3 replicates.
Step two: full-charge shallow-discharge test:
and (3) placing the soft package full cell in a constant temperature box at 45 ℃. Charging to an upper limit voltage of 4.45V by adopting a charging rate current of 0.5C and constant current, then charging to a cut-off current of 0.05C by adopting constant voltage so as to enable the SoC to reach about 100%, and standing for 10min; discharging with 0.05C discharge rate current for 60min to 95% target SoC, standing for 10min; repeating the above steps until the battery produces gas, and recording the cycle number of the battery during gas production. The results are shown in Table 1.
TABLE 1 number of full charge and short discharge cycles of positive electrode materials of different process numbers in comparative example 1
| Positive electrode material | Number of cycles |
| A | 805 |
| B | 739 |
| C | 654 |
| D | 376 |
The LiCoO prepared by the evaluation methods provided in examples 1 to 4 respectively for the four process numbers A, B, C, D 2 The results of the detection evaluation of the positive electrode material are shown in table 2.
TABLE 2 test results of examples
As can be seen from the results in tables 1 and 2, the cycle number actually achieved by the high-temperature full charge and shallow discharge of the positive electrode material is strongly related to the metal element elution amount of the positive electrode material, the cycle number is high during gas production of the soft package full cell, and the elution amount of the metal element test corresponding to the corresponding button half cell is small.
The result shows that the evaluation method provided by the embodiment of the invention can effectively and qualitatively determine the quality of the high-temperature full-charge shallow-discharge performance of the cathode material. The method can greatly shorten the period of testing the full-cell full-charge shallow-discharge performance, does not need to wait for the gas production of an excessively high cycle number and then confirm the full-charge shallow-discharge performance, can directly judge the full-cell full-charge shallow-discharge performance according to the dissolution amount of the metal elements through a small cycle number, and is favorable for quickly and qualitatively evaluating the high-temperature full-charge shallow-discharge performance of the cathode material. In addition, the higher the test environment temperature is, the higher the charging voltage is, the higher the metal element elution amount in the positive electrode material is, and the rule is consistent, so that the parameters such as the environment temperature and the charging voltage of the cycle test can be properly improved in the actual operation, and the test period is further shortened.
The present application has been described in detail with reference to the embodiments, but the present application is not limited to the embodiments described above, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present application. Furthermore, the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
Claims (7)
1. The method for evaluating the high-temperature full-charge and shallow-discharge performance of the lithium battery positive electrode material is characterized by comprising the following steps of:
the method comprises the following steps: preparing a lithium battery anode material into a battery;
step two: charging the battery to 4.2V to 4.6V at a constant current with a charging rate current of 0.2C to 1.5C at a temperature of 45-55 ℃, and then charging the battery to a cut-off current of 0.01C to 0.1C at a constant voltage, so that the battery is charged to about 100 percent SoC; discharging the battery at a discharge rate current of 0.05C for 60min to 95% of a target SoC; repeating for n times;
step three: disassembling the battery, and cleaning the battery assembly by using an organic solvent to obtain a solution of a dissolved matter; judging the full charge and shallow discharge performance of the lithium battery positive electrode material according to the content of the metal element in the dissolved matter, wherein the metal element is selected from at least one of nickel, cobalt and manganese;
wherein the battery is a button type half battery, and n is more than or equal to 50 and less than or equal to 500.
2. The evaluation method according to claim 1, wherein the charge multiplying current is 0.5C to 1.0C; the upper limit voltage is 4.3V-4.5V; the cutoff current is 0.02C to 0.05C.
3. The evaluation method according to claim 1, wherein in the second step, the charging is performed to 100% of the SoC, and the charging is performed for 1min to 20min, and the discharging is performed to the target SoC, and the charging is performed for 1min to 20min.
4. The evaluation method according to claim 3, wherein in the second step, the charging is performed to 100% SoC and then the charging is performed for 5min to 15min, and the charging is performed to the target SoC and then the charging is performed for 5min to 15min.
5. The evaluation method according to any one of claims 1 to 4, wherein the organic solvent is at least one selected from the group consisting of ethylene carbonate, dimethyl carbonate, diethyl carbonate, propylene carbonate, and ethyl methyl carbonate.
6. The evaluation method according to any one of claims 1 to 4, wherein the battery is discharged to 2.5V to 3.5V before the eluate of the battery is collected.
7. The evaluation method according to any one of claims 1 to 4, wherein the detection method of the metal element is inductively coupled plasma atomic emission spectrometry.
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| CN114551865A (en) * | 2022-02-18 | 2022-05-27 | 惠州市豪鹏科技有限公司 | Rapid characterization method, comparison method and pretreatment reagent for cycle performance of lithium cobaltate |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103022552A (en) * | 2012-12-20 | 2013-04-03 | 中国东方电气集团有限公司 | Long-life lithium ion battery used under shallow charging and discharging conditions and preparation method of same |
| CN105580190A (en) * | 2013-09-25 | 2016-05-11 | 国立大学法人东京大学 | Electrolyte solution for electricity storage devices such as batteries and capacitors containing salt, wherein alkali metal, alkaline earth metal or aluminum serves as cations, and organic solvent having hetero element, method for producing same, and capacitor provided with said electrolyte solution |
| KR20170073163A (en) * | 2015-12-18 | 2017-06-28 | 주식회사 엘지화학 | Method for testing cycle life of positive electrode active material for secondary battery |
| CN107565098A (en) * | 2016-06-30 | 2018-01-09 | 河南科隆新能源股份有限公司 | A kind of Fast Evaluation anode material for lithium-ion batteries stability approach |
| CN107768708A (en) * | 2017-08-28 | 2018-03-06 | 天津力神电池股份有限公司 | The fast appraisement method of lithium battery graphite cathode material cycle performance |
| CN109004288A (en) * | 2018-08-16 | 2018-12-14 | 皖西学院 | A kind of high SOC of lithium battery low current disturbance nearby circulation chemical synthesizing method |
| CN109581240A (en) * | 2018-11-29 | 2019-04-05 | 北京航空航天大学 | Lithium ion battery failure analysis method based on AC impedence method |
| CN109709493A (en) * | 2018-12-29 | 2019-05-03 | 北京长城华冠汽车科技股份有限公司 | The test method and test macro of service life of lithium battery |
| CN111913117A (en) * | 2020-08-04 | 2020-11-10 | 中国科学院物理研究所 | Positive pole piece safety detection method |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103454589B (en) * | 2012-06-04 | 2016-01-27 | 中国科学院深圳先进技术研究院 | The performance of battery module detection method of electric automobile |
| CN103018683A (en) * | 2012-12-24 | 2013-04-03 | 天津力神电池股份有限公司 | Battery cycle performance accelerating and evaluating method |
| CN103529395B (en) * | 2013-10-25 | 2016-03-30 | 长城汽车股份有限公司 | The cold start power evaluation method of power battery pack |
| JP6848394B2 (en) * | 2016-03-22 | 2021-03-24 | 住友金属鉱山株式会社 | Lithium-ion secondary battery characterization method and lithium-ion secondary battery |
| CN108267693B (en) * | 2017-01-01 | 2019-07-26 | 北京当升材料科技股份有限公司 | A kind of fast appraisement method of anode material of lithium battery high-temperature storage performance |
| CN109459463B (en) * | 2017-12-05 | 2021-06-22 | 北京当升材料科技股份有限公司 | Rapid evaluation method for thermal storage stability of lithium ion battery positive electrode material |
| CN110108698A (en) * | 2019-04-24 | 2019-08-09 | 宜宾锂宝新材料有限公司 | A kind of performance judgment method of anode material for lithium-ion batteries |
| CN110726940B (en) * | 2019-09-19 | 2021-10-01 | 深圳市比克动力电池有限公司 | Method for rapidly evaluating cycle performance of high-nickel cathode material of lithium ion battery |
| CN114583277A (en) * | 2020-03-27 | 2022-06-03 | 宁德新能源科技有限公司 | Electrochemical device and electronic device including the same |
-
2020
- 2020-12-25 CN CN202011566913.1A patent/CN112731174B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103022552A (en) * | 2012-12-20 | 2013-04-03 | 中国东方电气集团有限公司 | Long-life lithium ion battery used under shallow charging and discharging conditions and preparation method of same |
| CN105580190A (en) * | 2013-09-25 | 2016-05-11 | 国立大学法人东京大学 | Electrolyte solution for electricity storage devices such as batteries and capacitors containing salt, wherein alkali metal, alkaline earth metal or aluminum serves as cations, and organic solvent having hetero element, method for producing same, and capacitor provided with said electrolyte solution |
| KR20170073163A (en) * | 2015-12-18 | 2017-06-28 | 주식회사 엘지화학 | Method for testing cycle life of positive electrode active material for secondary battery |
| CN107565098A (en) * | 2016-06-30 | 2018-01-09 | 河南科隆新能源股份有限公司 | A kind of Fast Evaluation anode material for lithium-ion batteries stability approach |
| CN107768708A (en) * | 2017-08-28 | 2018-03-06 | 天津力神电池股份有限公司 | The fast appraisement method of lithium battery graphite cathode material cycle performance |
| CN109004288A (en) * | 2018-08-16 | 2018-12-14 | 皖西学院 | A kind of high SOC of lithium battery low current disturbance nearby circulation chemical synthesizing method |
| CN109581240A (en) * | 2018-11-29 | 2019-04-05 | 北京航空航天大学 | Lithium ion battery failure analysis method based on AC impedence method |
| CN109709493A (en) * | 2018-12-29 | 2019-05-03 | 北京长城华冠汽车科技股份有限公司 | The test method and test macro of service life of lithium battery |
| CN111913117A (en) * | 2020-08-04 | 2020-11-10 | 中国科学院物理研究所 | Positive pole piece safety detection method |
Non-Patent Citations (3)
| Title |
|---|
| G. Lutzemberger et.al.Cycle life evaluation of lithium cells subjected to micro-cycles.《2015 5th International Youth Conference on Energy (IYCE)》.2015,第1-5页. * |
| 嘉红霞 等.《港口智能控制》.上海科学技术出版社,2017,第234页. * |
| 王其钰 等.锂离子电池失效分析概述.《储能科学与技术》.2017,第6卷(第5期),第1008-1025页. * |
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